CN113491791A - Heparin-loaded micro-nano composite fiber membrane and preparation method thereof - Google Patents

Heparin-loaded micro-nano composite fiber membrane and preparation method thereof Download PDF

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Publication number
CN113491791A
CN113491791A CN202010252517.5A CN202010252517A CN113491791A CN 113491791 A CN113491791 A CN 113491791A CN 202010252517 A CN202010252517 A CN 202010252517A CN 113491791 A CN113491791 A CN 113491791A
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pcl
pvp
heparin
fiber membrane
micro
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张兴光
王威
王杰
郭丁丁
陈星�
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Suzhou Hexiang Textile Technology Co ltd
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Suzhou Hexiang Textile Technology Co ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/26—Mixtures of macromolecular compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54—Biologically active materials, e.g. therapeutic substances
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/58—Materials at least partially resorbable by the body
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/04—Macromolecular materials
    • A61L31/041—Mixtures of macromolecular compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L31/148—Materials at least partially resorbable by the body
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L31/16—Biologically active materials, e.g. therapeutic substances
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/04—Dry spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30—Conjugate filaments; Spinnerette packs therefor
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/005—Synthetic yarns or filaments
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
    • D04H3/02—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of forming fleeces or layers, e.g. reorientation of yarns or filaments
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/23—Carbohydrates
    • A61L2300/236—Glycosaminoglycans, e.g. heparin, hyaluronic acid, chondroitin
    • A—HUMAN NECESSITIES
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    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/41—Anti-inflammatory agents, e.g. NSAIDs
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces

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Abstract

The application relates to a micro-nano composite fiber membrane and a preparation method thereof. The PCL/PVP composite micro-nano fiber membrane loaded with heparin is prepared by a solution jet spinning technology for the first time, and has the advantages of smooth surface, uniform diameter, high bioactivity and the like.

Description

Heparin-loaded micro-nano composite fiber membrane and preparation method thereof
Technical Field
The application belongs to the field of preparation of biomedical materials, relates to a heparin-loaded micro-nano composite fiber membrane, and particularly relates to a heparin-loaded micro-nano composite fiber membrane prepared by adopting a solution jet spinning technology.
Background
The collagen has good biocompatibility, good moisturizing hydrophilicity and degradability, and better effects of inducing cell adhesion, differentiation and propagation, is a natural high polymer material, is widely applied to the field of biomedical materials, but has low strength and no water solubility, and the polyvinyl alcohol and the polyvinylpyrrolidone are another biomedical material used for a long time and have the advantages of good spinnability, good water solubility, high strength and the like. The polyvinyl alcohol and the polyvinylpyrrolidone are blended with the collagen, so that the defect of insufficient strength of the collagen can be made up to a certain extent. The heparin has anticoagulant, antiinflammatory, and antiallergic effects, and can enhance affinity of antithrombin 3 and thrombin, accelerate thrombin inactivation, inhibit adhesion and aggregation of platelet, enhance activity of protein c, and stimulate vascular endothelial cells to release anticoagulant and fibrinolytic substances. Also has the functions of inhibiting blood platelets, increasing the permeability of the vascular wall, regulating angiogenesis and regulating blood fat, and is widely applied clinically.
The solution jet spinning technology is a novel method for preparing micro-nano fibers, and compared with the traditional electrostatic spinning method, the method does not need an electric field environment, does not need high-voltage equipment or any conductive collector, is simpler in equipment, can be used for spinning at a higher injection speed, is easy to operate, is low in cost, and is higher in spinning efficiency. The polymer has wider selection range, is not limited to the polymer with higher dielectric constant, and adopts the solvent which is easy to volatilize, has no toxicity and is more environment-friendly. The solution jet spinning technique is to deposit fibers on a substrate or a support surface by dissolving a polymer in a volatile solvent and treating the polymer solution with a pressurized gas flowing at a high speed to promote volatilization of the solvent and deposition refinement of the fibers. The prepared micro-nanofiber has wide commercial value, and can be applied to polymer reinforcement, medical treatment, PM2.5 filtration, electrical and optical devices and the like.
The invention prepares the micro-nano fiber by a simple, rapid and efficient solution jet spinning technology, fully utilizes the biological property of collagen and the mechanical property of polyvinyl alcohol to achieve the effect of complementary advantages, and the obtained material can be widely used in the fields of biomedical materials, sensor materials, filtering materials, bionics and the like.
Disclosure of Invention
In order to solve the above problems, the following technical solutions have been proposed through intensive research.
A micro-nano composite fiber membrane prepared by adopting a solution jet spinning technology is characterized in that: this nanofiber material is by polycaprolactone PCL, polyvinylpyrrolidone PVP, I type collagen and heparin as raw materials, and the PCL/PVP complex of load heparin is received through solution spray spinning technique preparation and is received the fibrous membrane a little, and wherein, the concentration of heparin is 5 ~ 20mg/ml, according to weight parts, PCL: 1-10% of PVP: 10-1, the type I collagen adopts an acetic acid solution of collagen, the concentration of the acetic acid solution is 0.2-0.6 wt%, the fiber diameter is 10 nm-0.8 mu m, and the fiber specific surface area is 150-185 m2And/g, the cytotoxicity reaction of the micro-nano composite fiber membrane is not more than 1 grade.
Preferably, the concentration of the heparin is 8-17 mg/ml, and the weight parts of the heparin are as follows: PVP is 2-7: 8-3.
Preference is given toThe diameter of the fiber is 50-690 nm, and the specific surface area of the fiber is 160-175 m2/g。
Preferably, the concentration of the acetic acid solution of type I collagen is 0.5 wt%.
A preparation method of a PCL/PVP composite micro-nano fiber membrane loaded with heparin comprises the following steps:
(1) according to parts by weight of PCL: 1-10% of PVP: 10-1, weighing polycaprolactone PCL and polyvinylpyrrolidone PVP, carrying out vacuum drying, adding the PCL and the PVP into an organic solvent, carrying out ultrasonic stirring at 45 ℃ until the PCL and the PVP are uniformly mixed, adding heparin with the concentration of 5-20 mg/ml and I-type collagen acetic acid solution with the concentration of 0.2-0.6 wt%, and carrying out ultrasonic stirring to obtain uniform dispersion liquid, namely polymer spray spinning stock solution; the organic solvent is any one of dichloromethane, ethanol, ethyl acetate and acetone;
(2) metering the polymer jet spinning stock solution prepared in the step (1) by a metering pump, feeding the polymer jet spinning stock solution into a spinning nozzle, extruding the polymer jet spinning stock solution from a spinning nozzle to form a trickle, and simultaneously carrying out high-speed air flow blowing and stretching on the trickle by adopting a spraying device to obtain a PCL/PVP composite micro-nano fiber membrane deposited on a substrate, wherein the air flow pressure is 50-80 psi;
(3) airing the nanofiber membrane prepared in the step (2) on an aseptic clean workbench, and adopting the dosage of 10-20 KGy/h60And (3) carrying out disinfection and sterilization treatment on gamma rays generated by Co, and forming and packaging to obtain the PCL/PVP composite micro-nano fiber membrane loaded with heparin.
Preferably, the concentration of the heparin is 8-17 mg/ml, and the weight parts of the heparin are as follows: PVP is 2-7: 8-3, wherein the concentration of the acetic acid solution of the type I collagen is 0.5 wt%.
Preferably, the gas stream pressure in step (1) is 70 psi.
Preferably, the diameter of the fiber is 50-690 nm, and the specific surface area of the fiber is 160-175 m2/g。
Advantageous effects
The technical scheme provided by the invention has the beneficial effects that: the invention firstly prepares a PCL/PVP composite micro-nano fiber membrane loaded with heparin through a solution spraying and spinning technology, and the PCL/PVP composite micro-nano fiber membrane has the advantages of smooth surface, uniform diameter, high biological activity and the like, the PCL and PVP polymers are subjected to phase separation in the solution spraying and spinning process due to different solubilities, through holes with nanoscale sizes can be formed on the surface and in the nanofiber membrane prepared through the solution spraying and spinning technology, the through holes are mutually communicated to form a network structure, the specific surface area of the nanofiber is further increased, the growth and the proliferation of cells are facilitated, the heparin has the excellent characteristics of anticoagulation, anti-inflammation and anti-allergy effects, and according to a synergistic theory, the composite membrane simultaneously has the performances of good hydrophilicity, biodegradability and the like of a PCL/PVP composite membrane, and has excellent biological activity of collagen, and has the anticoagulation property of the heparin, Has anti-inflammatory and anti-allergic effects, and the like, has excellent biocompatibility and biodegradability, can be used for bone tissue engineering or used as a biological scaffold material, has various functions, is convenient for mass production, and has good application prospect.
Detailed Description
Example 1
A preparation method of a PCL/PVP composite micro-nano fiber membrane loaded with heparin comprises the following steps:
(1) according to parts by weight of PCL: PVP 5: 8, weighing polycaprolactone PCL and polyvinylpyrrolidone PVP according to the proportion, carrying out vacuum drying, adding PCL and PVP into a mixed organic solvent of dichloromethane and ethanol, carrying out ultrasonic stirring at 45 ℃ until the mixture is uniformly mixed, adding heparin with the concentration of 15mg/ml and I-type collagen acetic acid solution with the concentration of 0.4 wt%, and carrying out ultrasonic stirring to obtain uniform dispersion liquid, namely the polymer spray spinning stock solution.
(2) Metering the polymer jet spinning stock solution prepared in the step (1) by a metering pump, feeding the polymer jet spinning stock solution into a spinning nozzle, extruding the polymer jet spinning stock solution from a spinning nozzle to form a trickle, and simultaneously carrying out high-speed air flow blowing and stretching on the trickle by adopting a spraying device to obtain a PCL/PVP composite micro-nano fiber membrane deposited on a substrate, wherein the air flow pressure is 60 psi;
(3) airing the nanofiber membrane prepared in the step (2) on an aseptic clean workbench, and adopting the dosage of 15KGy/h60Gamma ray generated by CoAnd (4) sterilizing, forming and packaging to obtain the PCL/PVP composite micro-nano fiber membrane loaded with heparin. The fiber diameter is 453nm, and the specific surface area of the fiber is 165m2/g。
Example 2
A preparation method of a PCL/PVP composite micro-nano fiber membrane loaded with heparin comprises the following steps:
(1) according to parts by weight of PCL: PVP ═ 2: 5, weighing polycaprolactone PCL and polyvinylpyrrolidone PVP according to the proportion, carrying out vacuum drying, adding PCL and PVP into a mixed organic solvent of dichloromethane and ethanol, carrying out ultrasonic stirring at 45 ℃ until the mixture is uniformly mixed, then adding heparin with the concentration of 18mg/ml and I-type collagen acetic acid solution with the concentration of 0.5 wt%, and carrying out ultrasonic stirring to obtain uniform dispersion liquid, namely the polymer spray spinning stock solution.
(2) Metering the polymer jet spinning stock solution prepared in the step (1) by a metering pump, feeding the polymer jet spinning stock solution into a spinning nozzle, extruding the polymer jet spinning stock solution from a spinning nozzle to form a trickle, and simultaneously carrying out high-speed air flow blowing and stretching on the trickle by adopting a spraying device to obtain a PCL/PVP composite micro-nano fiber membrane deposited on a substrate, wherein the air flow pressure is 70 psi;
(3) airing the nanofiber membrane prepared in the step (2) on an aseptic clean workbench, and adopting the dosage of 15KGy/h60And (3) carrying out disinfection and sterilization treatment on gamma rays generated by Co, and forming and packaging to obtain the PCL/PVP composite micro-nano fiber membrane loaded with heparin. The diameter of the fiber is 120nm, and the specific surface area of the fiber is 158m2/g。
Example 3
A preparation method of a nanofiber material for filtering heavy metal ions comprises the following steps:
a preparation method of a PCL/PVP composite micro-nano fiber membrane loaded with heparin comprises the following steps:
(1) according to parts by weight of PCL: PVP 8: 6, weighing polycaprolactone PCL and polyvinylpyrrolidone PVP according to the proportion, carrying out vacuum drying, adding PCL and PVP into a mixed organic solvent of dichloromethane and ethanol, carrying out ultrasonic stirring at 45 ℃ until the mixture is uniformly mixed, then adding heparin with the concentration of 18mg/ml and I-type collagen acetic acid solution with the concentration of 0.5 wt%, and carrying out ultrasonic stirring to obtain uniform dispersion liquid, namely the polymer spray spinning stock solution.
(2) Metering the polymer jet spinning stock solution prepared in the step (1) by a metering pump, feeding the polymer jet spinning stock solution into a spinning nozzle, extruding the polymer jet spinning stock solution from a spinning nozzle to form a trickle, and simultaneously carrying out high-speed air flow blowing and stretching on the trickle by adopting a spraying device to obtain a PCL/PVP composite micro-nano fiber membrane deposited on a substrate, wherein the air flow pressure is 75 psi;
(3) airing the nanofiber membrane prepared in the step (2) on an aseptic clean workbench, and adopting the dosage of 20KGy/h60And (3) carrying out disinfection and sterilization treatment on gamma rays generated by Co, and forming and packaging to obtain the PCL/PVP composite micro-nano fiber membrane loaded with heparin. The diameter of the fiber is 673nm, the specific surface area of the fiber is 179m2/g。
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (8)

1. A micro-nano composite fiber membrane prepared by adopting a solution jet spinning technology is characterized in that: this nanofiber material is by polycaprolactone PCL, polyvinylpyrrolidone PVP, I type collagen and heparin as raw materials, and the compound micro-nano fibrous membrane of PCL/PVP that obtains load heparin is prepared through solution spray spinning technique, and wherein, the concentration of heparin is 5 ~ 20mg/ml, according to weight parts, PCL: 1-10% of PVP: 10-1, the type I collagen adopts an acetic acid solution of collagen, the concentration of the acetic acid solution is 0.2-0.6 wt%, the fiber diameter is 10 nm-0.8 mu m, and the fiber specific surface area is 150-185 m2And/g, the cytotoxicity reaction of the micro-nano composite fiber membrane is not more than 1 grade.
2. The micro-nano composite fiber membrane prepared by adopting the solution jet spinning technology according to claim 1, wherein the concentration of the heparin is 8-17 mg/ml, and the weight parts of the heparin are as follows: PVP is 2-7: 8-3.
3. The micro-nano composite fiber membrane prepared by adopting the solution jet spinning technology according to the claims 1-2, wherein the fiber diameter is 50-690 nm, and the fiber specific surface area is 160-175 m2/g。
4. The micro-nano composite fiber membrane prepared by the solution jet spinning technology according to the claims 1-3, wherein the concentration of the acetic acid solution of the type I collagen is 0.5 wt%.
5. A preparation method of a PCL/PVP composite micro-nano fiber membrane loaded with heparin comprises the following steps:
(1) according to parts by weight of PCL: 1-10% of PVP: 10-1, weighing polycaprolactone PCL and polyvinylpyrrolidone PVP, carrying out vacuum drying, adding the PCL and the PVP into an organic solvent, carrying out ultrasonic stirring at 45 ℃ until the PCL and the PVP are uniformly mixed, adding heparin with the concentration of 5-20 mg/ml and I-type collagen acetic acid solution with the concentration of 0.2-0.6 wt%, and carrying out ultrasonic stirring to obtain uniform dispersion liquid, namely polymer spray spinning stock solution; the organic solvent is any one of dichloromethane, ethanol, ethyl acetate and acetone;
(2) metering the polymer jet spinning stock solution prepared in the step (1) by a metering pump, feeding the polymer jet spinning stock solution into a spinning nozzle, extruding the polymer jet spinning stock solution from a spinning nozzle to form a trickle, and simultaneously carrying out high-speed air flow blowing and stretching on the trickle by adopting a spraying device to obtain a PCL/PVP composite micro-nano fiber membrane deposited on a substrate, wherein the air flow pressure is 50-80 psi;
(3) airing the nanofiber membrane prepared in the step (2) on an aseptic clean workbench, and adopting the dosage of 10-20 KGy/h60And (3) carrying out disinfection and sterilization treatment on gamma rays generated by Co, and forming and packaging to obtain the PCL/PVP composite micro-nano fiber membrane loaded with heparin.
6. The preparation method of the PCL/PVP composite micro-nano fiber membrane loaded with heparin according to claim 5, wherein the concentration of the heparin is 8-17 mg/ml, and the weight ratio of PCL: PVP is 2-7: 8-3, wherein the concentration of the acetic acid solution of the type I collagen is 0.5 wt%.
7. The preparation method of the PCL/PVP composite micro-nano fiber membrane loaded with heparin according to claim 5, wherein the airflow pressure in the step (1) is 70 psi.
8. The preparation method of the PCL/PVP composite micro-nano fiber membrane loaded with heparin according to claim 5, wherein the diameter of the fiber is 50-690 nm, and the specific surface area of the fiber is 160-175 m2/g。
CN202010252517.5A 2020-04-01 2020-04-01 Heparin-loaded micro-nano composite fiber membrane and preparation method thereof Pending CN113491791A (en)

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